In this study, mixtures of trichloroisocyanuric acid (TCI) and fumaric acid (FA) solutions were applied to a difficult-to-bond, vulcanized styrene-butadiene rubber (R2) to analyze the combined effect of both surface treatments. The treated R2 rubber surfaces were characterized using advancing contact angle measurements, ATR-IR and XPS spectroscopy, and SEM. T-peel tests of treated R2 rubber/ polyurethane adhesive/leather joints have been obtained in order to quantify the adhesion properties. The wettability of R2 rubber was improved by treatment with 3 wt% TCI/EA (ethyl acetate) or 0.5 wt% FA/EtOH, and lower contact angles were obtained by treatment with both 3 wt% TCI/EA and 0.5 wt% FA/EtOH. The improved wettability was ascribed to the creation of carbon-chlorine moieties, the removal of zinc stearate and paraffin wax, and the creation of surface roughness on the R2 rubber surface. Treatment of R2 rubber with 3 wt% TCI/EA before or after treatment with 0.5 wt% FA/EtOH, or with a solution containing 3 wt% TCI/EA + 0.5 wt% FA/EtOH mixture produced a noticeable increase in peel strength. Always, the effects of the treatment of R2 rubber with 3 wt% TCI solution were dominant over those produced by treatment with 0.5 wt% FA solution in ethanol (FA/EtOH). On the other hand, the treatment of R2 rubber with 3 wt% TCI/EA + 0.5 wt% FA/EtOH mixture was more effective than the treatment with 0.5 wt% TCI/EA+ 2 wt% FA/EtOH because the lower amount of chlorinating agent in this mixture.